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Article(id=1215670314068005576, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1215670311140381365, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250331007, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1743350400000, receivedDateStr=2025-03-31, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1767767988935, onlineDateStr=2026-01-07, pubDate=1753372800000, pubDateStr=2025-07-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1767767988935, onlineIssueDateStr=2026-01-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1767767988935, creator=13701087609, updateTime=1767767988935, updator=13701087609, issue=Issue{id=1215670311140381365, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='14', pageStart='1', pageEnd='326', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1767767988237, creator=13701087609, updateTime=1767970098618, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1216518023599538606, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1215670311140381365, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1216518023599538607, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1215670311140381365, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=97, endPage=104, ext={EN=ArticleExt(id=1215670316144186161, articleId=1215670314068005576, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Fast detection of trace elements in aluminum foil by fiber laser induced breakdown spectroscopy, columnId=1215670315447931654, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Non-destructive Detection Technology in Food, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a safety, rapid, cost-effective and reliable analytical method for trace elements detection in aluminum foil based on fiber laser induced breakdown spectroscopy. Methods Using standards to evaluate analytical sensitivity and limit of detection of fiber laser induced breakdown spectroscopy after optimization of laser pulse width, pulse energy, repetition rate and baseline-correction, and the optimized method was applied to analyze trace elements in aluminum foil samples. Results Calibration curves for most elements achieved regression coefficients up to 0.99. Detection sensitivity and limit of detection followed the descending order of Mn>Cr>Cu>Ti>Mg>Fe>Zn>Si, and the average relative error of leave-one-out cross validation of all the elements was 14.45%. The detection results of 8 kinds of trace elements in 27 kinds of aluminum foil samples showed that Fe and Si were frequently detected, while Cu and Ti elements were rarely detected and Cr, Mg, Mn and Zn elements were not detected. Conclusion This method requires no sample preparation, offers rapid analysis speed, and enables simultaneous multi-element detection with high sensitivity, which promisingly makes it a reliable approach for rapid determination of trace elements in aluminum foil.

, correspAuthors=Shu-Di ZHANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Bin-Bin XU, Shu-Di ZHANG, Zhou-Yi XU, Zhi-Sen LIANG, Fang-Fang CHEN, Gui-Hong WANG), CN=ArticleExt(id=1215670319239582670, articleId=1215670314068005576, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=光纤激光诱导击穿光谱法快速测定铝箔纸中微量元素, columnId=1215670315653452572, journalTitle=食品安全质量检测学报, columnName=专题：食品无损检测技术, runingTitle=null, highlight=null, articleAbstract=

目的 建立基于光纤激光诱导击穿光谱技术的安全、快速、经济、可靠的铝箔纸中微量元素的检测方法。方法 使用标准物质评估经激光脉宽、能量、重复频率和扣基线优化后的激光诱导击穿光谱法的灵敏度和检出限, 应用于市售铝箔纸样品的检测, 分析样品中的微量元素含量。结果 大多数元素校准曲线回归系数可达0.99, 分析灵敏度与检出限从高到低的排序是锰(Mn)>铬(Cr)>铜(Cu)>钛(Ti)>镁(Mg)>铁(Fe)>锌(Zn)>硅(Si), 所有元素的留一法交叉验证平均相对误差为14.45%。27种铝箔纸样品的8种微量元素检测结果显示, Fe、Si元素检出概率高, Cu、Ti元素检出概率低, Cr、Mg、Mn、Zn元素均未检出。结论 本方法无需样品制备, 分析速度快, 同时可检测多种元素, 各元素的分析灵敏度均较高, 有望成为铝箔纸中微量元素的快速检测的可靠方法。

, correspAuthors=张书迪, authorNote=null, correspAuthorsNote=
*张书迪(1991—), 男, 博士, 副教授, 主要研究方向为光谱分析仪器及方法的开发。E-mail:
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徐彬彬(1989—), 女, 硕士, 实验师, 主要研究方向为光谱分析仪器及方法的开发。E-mail:

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徐彬彬(1989—), 女, 硕士, 实验师, 主要研究方向为光谱分析仪器及方法的开发。E-mail:

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Journal of Analytical Atomic Spectrometry, 2018, 33(12): 2203-2209., articleTitle=Femtosecond laser-ablation spark-induced breakdown spectroscopy and its application to the elemental analysis of aluminum alloys, refAbstract=null), Reference(id=1215686866830017091, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2023, volume=38, issue=5, pageStart=1032, pageEnd=1042, url=null, language=null, rfNumber=[28], rfOrder=31, authorNames=XU B, LIN Z, XU Z, journalName=Journal of Analytical Atomic Spectrometry, refType=null, unstructuredReference=XU B, LIN Z, XU Z, et al. Denoising preprocessing using novel wavelet threshold functions in laser-induced breakdown spectroscopy based on fiber laser[J]. Journal of Analytical Atomic Spectrometry, 2023, 38(5): 1032-1042., articleTitle=Denoising preprocessing using novel wavelet threshold functions in laser-induced breakdown spectroscopy based on fiber laser, refAbstract=null), Reference(id=1215686866972623435, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2023, volume=35, issue=1, pageStart=012021, pageEnd=null, url=null, language=null, rfNumber=[29], rfOrder=32, authorNames=LV C, ZHANG N, LIN Z, journalName=Journal of Laser Applications, refType=null, unstructuredReference=LV C, ZHANG N, LIN Z, et al. Determination of copper, magnesium, and manganese in aluminum alloys using laser-induced breakdown spectroscopy based on fiber laser ablation[J]. Journal of Laser Applications, 2023, 35(1): 012021., articleTitle=Determination of copper, magnesium, and manganese in aluminum alloys using laser-induced breakdown spectroscopy based on fiber laser ablation, refAbstract=null), Reference(id=1215686867081675343, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2022, volume=37, issue=10, pageStart=2082, pageEnd=2088, url=null, language=null, rfNumber=[30], rfOrder=33, authorNames=LIN Z, ZHANG N, XU Z, journalName=Journal of Analytical Atomic Spectrometry, refType=null, unstructuredReference=LIN Z, ZHANG N, XU Z, et al. Modified iterative wavelets for background removal in laser-induced breakdown spectroscopy based on fiber laser ablation[J]. Journal of Analytical Atomic Spectrometry, 2022, 37(10): 2082-2088., articleTitle=Modified iterative wavelets for background removal in laser-induced breakdown spectroscopy based on fiber laser ablation, refAbstract=null), Reference(id=1215686867157172820, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2025, volume=16, issue=5, pageStart=10, pageEnd=15, url=null, language=null, rfNumber=[31], rfOrder=34, authorNames=张书迪, 肖晴天, 梁志森, journalName=食品安全质量检测学报, refType=null, unstructuredReference=张书迪, 肖晴天, 梁志森, 等. 光纤激光诱导击穿光谱技术快速检测铝质食品包装中铬含量[J]. 食品安全质量检测学报, 2025, 16(5): 10-15., articleTitle=光纤激光诱导击穿光谱技术快速检测铝质食品包装中铬含量, refAbstract=null), Reference(id=1215686867241058905, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2025, volume=16, issue=5, pageStart=10, pageEnd=15, url=null, language=null, rfNumber=[31], rfOrder=35, authorNames=ZHANG SD, XIAO QT, LIANG ZS, journalName=Journal of Food Safety & Quality, refType=null, unstructuredReference=ZHANG SD, XIAO QT, LIANG ZS, et al. Rapid determination of chromium in aluminum food packaging by fiber laser induced breakdown spectroscopy[J]. Journal of Food Safety & Quality, 2025, 16(5): 10-15., articleTitle=Rapid determination of chromium in aluminum food packaging by fiber laser induced breakdown spectroscopy, refAbstract=null), Reference(id=1215686867337527900, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2014, volume=99, issue=null, pageStart=138, pageEnd=149, url=null, language=null, rfNumber=[32], rfOrder=36, authorNames=YAROSHCHYK P, EBERHARDT JE, journalName=Spectrochimica Acta Part B: Atomic Spectroscopy, refType=null, unstructuredReference=YAROSHCHYK P, EBERHARDT JE. Automatic correction of continuum background in laser-induced breakdown spectroscopy using a model-free algorithm[J]. 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Analytica Chimica Acta, 2019, 8(1064): 11-16., articleTitle=Accuracy improvement of quantitative analysis for major elements in laser-induced breakdown spectroscopy using single-sample calibration, refAbstract=null), Reference(id=1215686867530465893, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2024, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[34], rfOrder=38, authorNames=肖昌乐, journalName=Al-Fe-Si电池箔制造过程中微观组织演变及性能研究, refType=null, unstructuredReference=肖昌乐. Al-Fe-Si电池箔制造过程中微观组织演变及性能研究[D]. 南京: 南京信息工程大学, 2024., articleTitle=null, refAbstract=null), Reference(id=1215686867715015272, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, doi=null, pmid=null, pmcid=null, year=2024, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[34], rfOrder=39, authorNames=XIAO CL, journalName=Study on the microstructural evolution and properties of Al-Fe-Si battery foil during manufacturing process, refType=null, unstructuredReference=XIAO CL. Study on the microstructural evolution and properties of Al-Fe-Si battery foil during manufacturing process[D]. 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Mass concentration of each element in the aluminum alloy standards (%)

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标准品编号 Cr Cu Fe Mg Mn Si Ti Zn
ZBY523a 0.2570 0.2900 0.546 1.0000 0.0940 0.640 0.0220 0.0170
ZBY524a 0.0200 0.0710 0.187 0.5400 0.0550 0.419 0.0055 0.0130
ZBY528 0.0007 0.0006 0.086 0.0072 0.0014 0.046 0.0097 0.0028
ZBY531 0.0150 0.2430 0.284 0.5410 0.0530 9.380 0.0500 0.0720
ZBY533 0.0025 1.0700 0.215 0.4000 0.3940 7.940 0.2040 0.0032
ZBY534 0.0320 2.0900 1.330 0.0320 0.2100 10.330 0.0470 0.2170
ZBY538 0.0022 0.0900 0.396 0.0046 1.0800 0.079 0.0360 0.0033
ZBY540 0.0012 0.0057 0.082 0.5990 0.0016 0.509 0.0160 0.0026
), ArticleFig(id=1215686858944725297, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=CN, label=表1, caption=

铝合金标准品中各元素的质量浓度(%)

, figureFileSmall=null, figureFileBig=null, tableContent=
标准品编号 Cr Cu Fe Mg Mn Si Ti Zn
ZBY523a 0.2570 0.2900 0.546 1.0000 0.0940 0.640 0.0220 0.0170
ZBY524a 0.0200 0.0710 0.187 0.5400 0.0550 0.419 0.0055 0.0130
ZBY528 0.0007 0.0006 0.086 0.0072 0.0014 0.046 0.0097 0.0028
ZBY531 0.0150 0.2430 0.284 0.5410 0.0530 9.380 0.0500 0.0720
ZBY533 0.0025 1.0700 0.215 0.4000 0.3940 7.940 0.2040 0.0032
ZBY534 0.0320 2.0900 1.330 0.0320 0.2100 10.330 0.0470 0.2170
ZBY538 0.0022 0.0900 0.396 0.0046 1.0800 0.079 0.0360 0.0033
ZBY540 0.0012 0.0057 0.082 0.5990 0.0016 0.509 0.0160 0.0026
), ArticleFig(id=1215686859062165819, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=EN, label=Table 2, caption=

Commercial information of 27 kinds of aluminum foil brands

, figureFileSmall=null, figureFileBig=null, tableContent=
编号 品牌 编号 品牌 编号 品牌
1 美嘉南 10 佳能 19 妙玛
2 皓原 11 马大帅 20 Labshark
3 展艺 12 茶花 21 炊大皇
4 洁成 13 法禧龙 22 好媳妇
5 妙洁 14 美丽雅 23 尚烤佳
6 旭包鲜 15 麦思琪 24 巴比客
7 Heavy Duty 16 和生 25 东洋
8 佳得美 17 箔洱特 26 悦心可
9 克林莱 18 优奥 27 Biosharp
), ArticleFig(id=1215686859158634815, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=CN, label=表2, caption=

27种铝箔纸品牌信息

, figureFileSmall=null, figureFileBig=null, tableContent=
编号 品牌 编号 品牌 编号 品牌
1 美嘉南 10 佳能 19 妙玛
2 皓原 11 马大帅 20 Labshark
3 展艺 12 茶花 21 炊大皇
4 洁成 13 法禧龙 22 好媳妇
5 妙洁 14 美丽雅 23 尚烤佳
6 旭包鲜 15 麦思琪 24 巴比客
7 Heavy Duty 16 和生 25 东洋
8 佳得美 17 箔洱特 26 悦心可
9 克林莱 18 优奥 27 Biosharp
), ArticleFig(id=1215686859292852550, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=EN, label=Table 3, caption=

Relationship between adjustable pulse width and energy of fiber laser

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脉宽/ns 最大
能量/mJ		 触发
频率/kHz		 脉宽/ns 最大
能量/mJ		 触发
频率/kHz
1 0.033 1500 45 0.556 90
2 0.056 900 60 0.625 80
4 0.089 560 80 0.714 70
6 0.125 400 100 0.769 65
9 0.167 300 150 2.083 24
13 0.238 210 200 2.500 20
20 0.333 150 250 2.941 17
30 0.455 110 350 4.167 12
), ArticleFig(id=1215686859414487375, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=CN, label=表3, caption=

光纤激光器可调脉宽与能量之间的关系

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脉宽/ns 最大
能量/mJ		 触发
频率/kHz		 脉宽/ns 最大
能量/mJ		 触发
频率/kHz
1 0.033 1500 45 0.556 90
2 0.056 900 60 0.625 80
4 0.089 560 80 0.714 70
6 0.125 400 100 0.769 65
9 0.167 300 150 2.083 24
13 0.238 210 200 2.500 20
20 0.333 150 250 2.941 17
30 0.455 110 350 4.167 12
), ArticleFig(id=1215686859540316503, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=EN, label=Table 4, caption=

LOD for 8 kinds of trace elements in aluminum sample

, figureFileSmall=null, figureFileBig=null, tableContent=
Cr Cu Fe Mg Mn Si Ti Zn
灵敏度S 415158 358198 50785 60501 630357 29795 127369 32870
噪音σ 12.48 12.88 15.03 15.86 17.02 17.99 17.99 15.49
LOD/(μg/g) 0.90 1.08 8.88 7.87 0.81 18.11 4.24 14.14
), ArticleFig(id=1215686860878299491, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=CN, label=表4, caption=

铝样品中8种微量元素LOD

, figureFileSmall=null, figureFileBig=null, tableContent=
Cr Cu Fe Mg Mn Si Ti Zn
灵敏度S 415158 358198 50785 60501 630357 29795 127369 32870
噪音σ 12.48 12.88 15.03 15.86 17.02 17.99 17.99 15.49
LOD/(μg/g) 0.90 1.08 8.88 7.87 0.81 18.11 4.24 14.14
), ArticleFig(id=1215686861012517224, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=EN, label=Table 5, caption=

Averaged relative error of each trace element (%)

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Cr Cu Fe Mg Mn Si Ti Zn
ARE 8.15 13.95 22.29 12.83 2.75 17.12 15.82 22.7
), ArticleFig(id=1215686861113180523, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=CN, label=表5, caption=

各微量元素平均相对偏差(%)

, figureFileSmall=null, figureFileBig=null, tableContent=
Cr Cu Fe Mg Mn Si Ti Zn
ARE 8.15 13.95 22.29 12.83 2.75 17.12 15.82 22.7
), ArticleFig(id=1215686861226426738, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=EN, label=Table 6, caption=

Content of 8 kinds of trace elements detected in 27 kinds of brands of aluminum foil samples (μg/g)

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 Cr Cu Fe Mg Mn Si Ti Zn
1 N.D. N.D. 989.78±179.39 N.D. N.D. 692.03±59.83 N.D. N.D.
2 N.D. N.D. 1639.89±309.57 N.D. N.D. 1377.40±258.88 N.D. N.D.
3 N.D. N.D. N.D. N.D. N.D. 500.69±76.28 N.D. N.D.
4 N.D. 14.78±3.57 1701.77±244.61 N.D. N.D. 1234.26±240.53 N.D. N.D.
5 N.D. 18.28±6.70 10.33±4.09 N.D. N.D. 410.27±92.24 N.D. N.D.
6 N.D. 69.60±14.75 557.39±92.84 N.D. N.D. 1258.52±242.58 N.D. N.D.
7 N.D. N.D. 1479.02±148.31 N.D. N.D. 1337.96±240.43 N.D. N.D.
8 N.D. 8.43±4.71 N.D. N.D. N.D. 548.83±114.92 N.D. N.D.
9 N.D. 30.62±8.05 N.D. N.D. N.D. 553.66±83.24 N.D. N.D.
10 N.D. 3.57±6.48 N.D. N.D. N.D. 443.16±123.44 N.D. N.D.
11 N.D. N.D. N.D. N.D. N.D. 374.76±82.08 N.D. N.D.
12 N.D. 188.16±36.07 2733.83±336.05 N.D. N.D. 1649.33±191.53 46.28±17.85 N.D.
13 N.D. 5.40±4.00 1906.21±324.68 N.D. N.D. 1587.95±362.79 N.D. N.D.
14 N.D. N.D. N.D. N.D. N.D. 462.74±129.88 N.D. N.D.
15 N.D. N.D. 343.61±52.96 N.D. N.D. 1045.31±175.07 N.D. N.D.
16 N.D. 7.24±6.53 49.86±15.88 N.D. N.D. N.D. N.D. N.D.
17 N.D. N.D. 495.75±28.16 N.D. N.D. 832.04±122.82 N.D. N.D.
18 N.D. 121.67±29.52 2207.98±433.86 N.D. N.D. 906.65±104.08 N.D. N.D.
19 N.D. N.D. 111.35±27.45 N.D. N.D. N.D. N.D. N.D.
20 N.D. 21.96±6.45 3005.57±590.74 N.D. N.D. 1913.09±261.54 61.94±15.97 N.D.
21 N.D. N.D. N.D. N.D. N.D. 450.14±91.11 N.D. N.D.
22 N.D. N.D. 1418.49±211.96 N.D. N.D. 1182.18±207.93 N.D. N.D.
23 N.D. N.D. 2149.00±220.57 N.D. N.D. 1106.53±261.21 N.D. N.D.
24 N.D. 8.95±2.63 282.57±29.22 N.D. N.D. 1120.68±155.99 N.D. N.D.
25 N.D. N.D. N.D. N.D. N.D. 543.53±78.44 N.D. N.D.
26 N.D. 2.98±1.63 N.D. N.D. N.D. 575.98±90.39 N.D. N.D.
27 N.D. N.D. 1919.40±344.48 N.D. N.D. 673.68±132.01 N.D. N.D.
), ArticleFig(id=1215686861373227383, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314068005576, language=CN, label=表6, caption=

27种铝箔纸样品的8种微量元素检测结果含量(μg/g)

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 Cr Cu Fe Mg Mn Si Ti Zn
1 N.D. N.D. 989.78±179.39 N.D. N.D. 692.03±59.83 N.D. N.D.
2 N.D. N.D. 1639.89±309.57 N.D. N.D. 1377.40±258.88 N.D. N.D.
3 N.D. N.D. N.D. N.D. N.D. 500.69±76.28 N.D. N.D.
4 N.D. 14.78±3.57 1701.77±244.61 N.D. N.D. 1234.26±240.53 N.D. N.D.
5 N.D. 18.28±6.70 10.33±4.09 N.D. N.D. 410.27±92.24 N.D. N.D.
6 N.D. 69.60±14.75 557.39±92.84 N.D. N.D. 1258.52±242.58 N.D. N.D.
7 N.D. N.D. 1479.02±148.31 N.D. N.D. 1337.96±240.43 N.D. N.D.
8 N.D. 8.43±4.71 N.D. N.D. N.D. 548.83±114.92 N.D. N.D.
9 N.D. 30.62±8.05 N.D. N.D. N.D. 553.66±83.24 N.D. N.D.
10 N.D. 3.57±6.48 N.D. N.D. N.D. 443.16±123.44 N.D. N.D.
11 N.D. N.D. N.D. N.D. N.D. 374.76±82.08 N.D. N.D.
12 N.D. 188.16±36.07 2733.83±336.05 N.D. N.D. 1649.33±191.53 46.28±17.85 N.D.
13 N.D. 5.40±4.00 1906.21±324.68 N.D. N.D. 1587.95±362.79 N.D. N.D.
14 N.D. N.D. N.D. N.D. N.D. 462.74±129.88 N.D. N.D.
15 N.D. N.D. 343.61±52.96 N.D. N.D. 1045.31±175.07 N.D. N.D.
16 N.D. 7.24±6.53 49.86±15.88 N.D. N.D. N.D. N.D. N.D.
17 N.D. N.D. 495.75±28.16 N.D. N.D. 832.04±122.82 N.D. N.D.
18 N.D. 121.67±29.52 2207.98±433.86 N.D. N.D. 906.65±104.08 N.D. N.D.
19 N.D. N.D. 111.35±27.45 N.D. N.D. N.D. N.D. N.D.
20 N.D. 21.96±6.45 3005.57±590.74 N.D. N.D. 1913.09±261.54 61.94±15.97 N.D.
21 N.D. N.D. N.D. N.D. N.D. 450.14±91.11 N.D. N.D.
22 N.D. N.D. 1418.49±211.96 N.D. N.D. 1182.18±207.93 N.D. N.D.
23 N.D. N.D. 2149.00±220.57 N.D. N.D. 1106.53±261.21 N.D. N.D.
24 N.D. 8.95±2.63 282.57±29.22 N.D. N.D. 1120.68±155.99 N.D. N.D.
25 N.D. N.D. N.D. N.D. N.D. 543.53±78.44 N.D. N.D.
26 N.D. 2.98±1.63 N.D. N.D. N.D. 575.98±90.39 N.D. N.D.
27 N.D. N.D. 1919.40±344.48 N.D. N.D. 673.68±132.01 N.D. N.D.
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光纤激光诱导击穿光谱法快速测定铝箔纸中微量元素
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徐彬彬 1 , 张书迪 1, * , 徐周毅 2 , 梁志森 3 , 陈芳芳 1 , 王贵弘 1
食品安全质量检测学报 | 专题：食品无损检测技术 2025,16(14): 97-104
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食品安全质量检测学报 | 专题：食品无损检测技术 2025, 16(14): 97-104
光纤激光诱导击穿光谱法快速测定铝箔纸中微量元素
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徐彬彬1 , 张书迪1, * , 徐周毅2, 梁志森3, 陈芳芳1, 王贵弘1
作者信息
  • 1 厦门医学院天然化妆品福建省高校工程研究中心, 厦门 361023
  • 2 厦门大学萨本栋微米纳米科学技术研究院, 厦门 361102
  • 3 广州检验检测认证集团有限公司, 广州 511447

    • 徐彬彬(1989—), 女, 硕士, 实验师, 主要研究方向为光谱分析仪器及方法的开发。E-mail:

通讯作者:

*张书迪(1991—), 男, 博士, 副教授, 主要研究方向为光谱分析仪器及方法的开发。E-mail:
Fast detection of trace elements in aluminum foil by fiber laser induced breakdown spectroscopy
Bin-Bin XU1 , Shu-Di ZHANG1, * , Zhou-Yi XU2, Zhi-Sen LIANG3, Fang-Fang CHEN1, Gui-Hong WANG1
Affiliations
  • 1 Engineering Research Center of Natural Cosmeceuticals College of Fujian Province, Xiamen Medical College, Xiamen 361023, China
  • 2 Peng-tung Sah Institute of Micro-Nano Science and Technology, Xiamen University, Xiamen 361102, China
  • 3 Guangzhou Inspection and Testing Certification Group Company Limited, Guangzhou 511447, China
出版时间: 2025-07-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250331007
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摘要
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目的 建立基于光纤激光诱导击穿光谱技术的安全、快速、经济、可靠的铝箔纸中微量元素的检测方法。方法 使用标准物质评估经激光脉宽、能量、重复频率和扣基线优化后的激光诱导击穿光谱法的灵敏度和检出限, 应用于市售铝箔纸样品的检测, 分析样品中的微量元素含量。结果 大多数元素校准曲线回归系数可达0.99, 分析灵敏度与检出限从高到低的排序是锰(Mn)>铬(Cr)>铜(Cu)>钛(Ti)>镁(Mg)>铁(Fe)>锌(Zn)>硅(Si), 所有元素的留一法交叉验证平均相对误差为14.45%。27种铝箔纸样品的8种微量元素检测结果显示, Fe、Si元素检出概率高, Cu、Ti元素检出概率低, Cr、Mg、Mn、Zn元素均未检出。结论 本方法无需样品制备, 分析速度快, 同时可检测多种元素, 各元素的分析灵敏度均较高, 有望成为铝箔纸中微量元素的快速检测的可靠方法。

光纤激光器  /  激光诱导击穿光谱  /  铝箔纸  /  快速检测  /  微量元素

Objective To establish a safety, rapid, cost-effective and reliable analytical method for trace elements detection in aluminum foil based on fiber laser induced breakdown spectroscopy. Methods Using standards to evaluate analytical sensitivity and limit of detection of fiber laser induced breakdown spectroscopy after optimization of laser pulse width, pulse energy, repetition rate and baseline-correction, and the optimized method was applied to analyze trace elements in aluminum foil samples. Results Calibration curves for most elements achieved regression coefficients up to 0.99. Detection sensitivity and limit of detection followed the descending order of Mn>Cr>Cu>Ti>Mg>Fe>Zn>Si, and the average relative error of leave-one-out cross validation of all the elements was 14.45%. The detection results of 8 kinds of trace elements in 27 kinds of aluminum foil samples showed that Fe and Si were frequently detected, while Cu and Ti elements were rarely detected and Cr, Mg, Mn and Zn elements were not detected. Conclusion This method requires no sample preparation, offers rapid analysis speed, and enables simultaneous multi-element detection with high sensitivity, which promisingly makes it a reliable approach for rapid determination of trace elements in aluminum foil.

fiber laser  /  laser induced breakdown spectroscopy  /  aluminum foil  /  fast detection  /  trace elements
徐彬彬, 张书迪, 徐周毅, 梁志森, 陈芳芳, 王贵弘. 光纤激光诱导击穿光谱法快速测定铝箔纸中微量元素. 食品安全质量检测学报, 2025 , 16 (14) : 97 -104 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250331007
Bin-Bin XU, Shu-Di ZHANG, Zhou-Yi XU, Zhi-Sen LIANG, Fang-Fang CHEN, Gui-Hong WANG. Fast detection of trace elements in aluminum foil by fiber laser induced breakdown spectroscopy[J]. Journal of Food Safety & Quality, 2025 , 16 (14) : 97 -104 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250331007
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0 引言
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铝箔纸常用作食品包装烹饪材料, 具有保温、防水、密封和传导的作用。不仅能帮助食物在烧烤、烘焙等烹调中均匀受热, 防止食物烧焦, 在食材的冷藏储存、密封保温、分隔热源等方面, 也能发挥作用, 极大提升了生活便利性, 受到广大消费者的欢迎[1]。铝箔纸由铝制成, 但生产过程中可能混有其他合金元素或杂质, 因此可能存在铅、镉等重金属超标的问题, 存在食品安全隐患[2-3]。铝箔生产时为达到某些性能要求(如拉伸强度、硬度、耐磨性、耐腐蚀性、电导率等)而可能添加一种或多种金属或非金属元素。其中金属合金元素如铝、铜(Cu)、铬(Cr)、锰(Mn)、钼、镍、锌(Zn)、锡、钴等; 非金属合金元素如碳、硅等。生产、加工过程中亦可能混有残留的非有意添加的杂质元素。GB 4806.9—2023《食品安全国家标准 食品接触用金属材料及制品》规定合金元素迁移量指标规定, Cr: 不得超过0.25 mg/kg, Cu: 不得超过4.00 mg/kg, Mn: 不得超过2.00 mg/kg, Zn: 不得超过5.00 mg/kg。铝及铝合金材料中金属基材和金属镀层中杂质元素含量要求砷不得超过0.01%(质量浓度), 镉、铅、汞总含量不得超过0.01%(质量浓度)。按照规定合金元素迁移量检测接触不同的食物及不同的烹饪方式的迁移实验方法均不同, 实验步骤烦琐且耗时。因此, 有必要开发铝箔纸中微量元素含量简便、快速的直接检测方法。安全标准中已明确规定Cr、Cu、Mn、Zn的要求, 虽未明确铁(Fe)、镁(Mg)、钛(Ti)、硅(Si)的含量要求, 但在铝合金的生产过程中亦常混有一定量的其他元素, 食用过量亦存在安全风险, 因此, 本研究对铝箔纸中Cr、Cu、Mn、Zn、Fe、Mg、Ti、Si 8种元素进行检测。
当前常用的检测方法有原子吸收分光光度法(atomic absorption spectrometry, AAS)、电感耦合等离子体-发射光谱法(inductively coupled plasma-optical emission spectrometry, ICP-OES)或电感耦合等离子体-质谱法(inductively coupled plasma-mass spectrometry, ICP-MS)[4]。这些方法虽具有稳定性好、适用范围广等优点, 但检测前需用大量强酸消解铝质金属样品, 容易产生环境污染, 且强酸与金属反应剧烈, 有一定的危险性。当检测样本量较大时, 因实验步骤较烦琐、耗时, 需要耗费大量时间和人力。另外, AAS、ICP-OES和ICP-MS等仪器较为昂贵, 使得样品检测成本较高。因此开发安全、高效、环保、经济的检测方法尤为重要。
激光诱导击穿光谱法(laser induced breakdown spectroscopy, LIBS)具有仪器结构简单、无需样品前处理、分析速度快、可原位分析等优点而被运用在材料科学[5-6]、法证鉴定[7-8]、地质学[9-10]、农业[11]、考古学[12]、生命科学[13]等广大领域中。光纤激光器是激光器的一种特定类型, 与传统的固体、气体或半导体激光器相比, 在结构、性能和应用上存在显著优势, 其具有价格低、光束质量高、可靠性高、操作及维护简单等优点。经过研究者们验证, 使用了光纤激光器的激光诱导击穿光谱法(fiber laser-laser induced breakdown spectrometry, FL-LIBS)在信噪比、校准曲线线性度和检出限(limit of detection, LOD)等分析效能参数上与普遍使用的灯泵浦固体激光器类似[14-17], 甚至能够获得更为简单谱图[18]。部分学者研究了进一步提高其检测灵敏度、LOD和分析准确度的方法, 如开发双激光架构[19-22]、额外引入电火花激发源[23-27]、开发扣背景算法等[28-30], 扩大了其使用范围, 促进了FL-LIBS的发展。但目前较少有基于FL-LIBS开发铝箔纸中微量元素的快速检测方法的报道。张书迪等[31]基于FL-LIBS开发了铝合金中重金属Cr的检测方法, 但尚未涉及其他微量元素的检测, 且定量分析性能有待进一步提高。本研究拟基于前期研究成果, 开发铝箔纸中其他微量元素的检测方法, 并进一步优化实验参数、提高检测能力, 为市面上铝箔纸样品中微量元素的快速检测提供准确、快速、绿色、经济的检测方案。
1 材料与方法
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1.1 材料与试剂
铝合金国家标准品ZBY523a、ZBY524a、ZBY528、ZBY531、ZBY533、ZBY534、ZBY538、ZBY540(济南众标科技有限公司), 各标准品中各元素含量如表1所示; 铝合金薄板(清河县宏昌金属材料有限公司); 27种不同品牌铝箔纸, 品牌信息如表2所示。
1.2 仪器与设备
1064 nm YDFLP-50-M8光纤激光器(深圳市杰普特光电股份有限公司); Y100WA 100*100电动二维移动平台(北京江云光电科技有限公司); HS2048四通道高分辨光纤光谱仪(上海如海光电科技有限公司)。
1.3 实验方法
(1)仪器架构
FL-LIBS分析平台架构如图1所示。相较前期研究而言, 本研究所用光纤激光器具备更高的单脉冲能量。激光脉冲经由反射镜反射后, 再经过聚焦透镜聚焦至样品表面产生等离子体, 其发射的光由4个芯径为600 μm的光纤线进行收集并传输至微型光纤光谱仪中(采集范围: 152~563 nm, 仪器半峰宽: 0.11 nm)。光纤激光器、微型光谱仪和二维移动平台的协同控制由自制电子控制卡进行控制。
(2) FL-LIBS实验方法
首先, 进行激光脉宽-能量综合优化。将铝合金薄板放在二维移动平台上, 并调节聚焦透镜位置使得激光聚焦于样品表面(焦距63 mm)。激光波长1064 nm, 触发频率如表3所示, 发射频率为3 Hz。设置二维移动平台以5 mm/s的速度进行连续移动, 移动距离15 mm, 光谱仪的积分时间为10 ms, 每个脉宽条件下, 分别使用其最高激光能量的40%、60%、80%、100%进行实验, 如表3所示。在每个实验条件下做50次平行实验。
其次, 根据上述实验结果, 选取最佳激光脉宽和能量参数, 进一步进行重复频率优化。激光频率设置为50、100、150、200、250、300、350、400 Hz, 单次实验中发射激光总个数为20个, 光谱积分时间1 s, 移动平台速度5 mm/s, 移动距离15 mm, 在每个实验条件下做50次平行实验。
最后, 对27种铝箔纸未知样品进行测量。对每份样品进行测定前, 事先用游标卡尺对其厚度进行测量, 并依此调整聚焦透镜位置, 使焦点始终位于样品表面。随后, 使用上述步骤中确定的最佳实验参数对每一份样品进行测量, 并收取光谱数据。对27种铝箔纸未知样品进行测量, 做50次平行实验。
1.4 数据处理
使用自行编写的Labview程序(v2020, 美国国家仪器有限公司)对FL-LIBS光谱数据进行扣基线、读取平均谱峰信号及计算标准偏差等初步处理操作, 使用Origin 2024软件对数据进行作图处理。在每个实验条件下做50次平行实验。
2 结果与分析
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2.1 FL-LIBS实验方法优化
2.1.1 基线评估与扣除
激光诱导等离子体在发生初期由于频繁的电子-电子碰撞会产生大量黑体辐射, 因此LIBS谱图通常有着很高的连续辐射信号, 如图2中黑色基线所示。过高的基线信号会对研究结果产生不利影响, 因此必须对实验结果进行扣基线优化处理。本研究采用YAROSHCHYK等[32]针对LIBS谱图开发的移动窗口最小值扣背景算法, 该算法因原理简单、计算速度快、处理效果好而被大量运用。其计算原理见式(1):
$B\left(i\right)={\displaystyle \sum \begin{array}{l}j=i+w/2\\ j=i-2/2+1\end{array}}\text{M}in(j)\times rect(i-j)$
式中: B(i)为最终拟合的背景曲线; i为谱图数据像素点序号; j为位于点i窗口处的数据像素点序号; w为移动窗口的长度(像素点个数); Min(j)为在该窗口内的数据最小值; rect(i-j)为方脉冲函数, 在窗口内的函数值为1/w, 而在窗口外的函数值为0。其中, B(i)、Min(j)、rect(i-j)的单位均为光谱信号强度值(任意单位, a.u.), i、j、w均为自然数(无单位)。
拟合结果如图2中红线所示, 背景线很好地贴合了原始谱图的整体底部。扣除基线后的谱图如图3所示, 可以看出, 扣除背景后谱图基线整体十分平缓且接近于0, 说明扣背景效果良好。本研究参考文献[23]选取各元素谱线并标注在图3中, 其均为各元素的常见特征谱线。
2.1.2 激光脉宽-能量综合优化
本研究中所用激光器可以对脉宽和能量进行调节, 依据激光器技术说明书设置以上两个参数, 其相对制约关系如表3所示。在每个脉宽下分别设置其最高能量的40%、60%、80%、100%进行参数优化探索, 结果如图4所示。从图4中可以看出, 同脉宽下信号随能量线性增长, 增长速度随脉宽变大而变慢, 但并非能量越大信号越强。信号强度同时取决于激光能量与脉宽, 理论上能量越大、脉宽越短(瞬时功率越强), 信号就越强。为了更清晰地展示最高信号强度的变化趋势, 将各个脉宽条件下可获得的最高信号强度数据取出并作图, 如图5所示。由图5可知, 脉宽低于30 ns时, 最高信号随着脉宽升高而迅速上升, 这主要是由于激光能量变大的原因, 使得溅射量提升、等离子体温度变高。脉宽增加至80 ns时, 最高信号缓慢上升, 随后开始明显下降。原因可能是脉宽的提升延长了热量的驰豫过程, 使得激发能量不能有效地聚集在被溅射的样品表面区域, 降低了能量的利用率。而当脉宽进一步提升至350 ns时, 最高信号强度又开始明显回升, 表明增强的激光能量抵消了长脉宽的热量驰豫影响, 在分析过程中重新占据了主导地位。综合以上讨论, 最高信号出现在80 ns, 故本研究使用80 ns、0.714 mJ作为后续实验条件。
2.1.3 重复频率优化
重复频率为激光脉冲每秒发射的次数, 不同的重复频率对信号强度有一定的影响。如图6所示, 总体随着重复频率上升, 信号有略微上升的趋势, 但影响程度相对较轻。理论上重复频率达到一定阈值后会产生明显的热量累积效应, 可以提高激光溅射量以及等离子体中分析物的粒子数量密度, 有助于分析信号的提升。本研究中重复频率影响较小, 可能的原因为所研究的重复频率范围较窄, 尚未达到热量累计效应发生所需要的阈值, 而本研究所使用的高能量光纤激光器由于其软硬件原因, 目前无法实现高于400 Hz的重复频率。综合以上结果, 选取400 Hz的条件做后续实验。
2.2 微量元素定量分析能力评估
各元素校准曲线由铝合金国家标准品测得, 结果如图7所示, 回归系数均高于0.94, 其中Cr、Mn元素回归系数最高, 可达0.9937。另外, 各元素的分析灵敏度(校准曲线斜率)如表4所示, 从高到低的排序是Mn>Cr>Cu>Ti>Mg>Fe>Zn>Si。其中灵敏度最高的是Mn元素。
为了进一步评估微量元素定量能力, 计算了各元素的LOD, 其表达式见式(2):
$\text{LOD}=3\sigma /S$
式中: σ为噪音的标准偏差, 即待测元素谱线周围的背景噪音数据的标准偏差值; S为该元素校准曲线的斜率。
各元素LOD如表4所示, 从高到低的排序是Mn>Cr>Cu>Ti>Mg>Fe>Zn>Si。Si是最低的, 是因为它是非金属元素, 电离能较高, 其原子、离子激发跃迁所需要的能量也较高, 所以同等条件下较难被激发而发射特征谱线。Mn是最高的, 是因为它的能级跃迁概率较高, 在等离子体冷却阶段(电子密度较低时)仍能保持较强信号。
为了评估方法的分析准确度, 本研究对各微量元素使用留一法交叉验证[33]并计算其平均相对误差(average relative error, ARE), 其表达式见式(3):
$\text{ARE}/\%=\frac{100}{n}{\displaystyle \sum \begin{array}{l}n\\ i=1\end{array}}\frac{|{\widehat{x}}_{i}-{x}_{i}|}{{x}_{i}}$
式中: n为样本数量, ${\widehat{x}}_{i}$为样本i的预测浓度, xi为样本i的实际浓度。
各元素平均相对偏差如表5所示, 从高到低的排序是Zn>Fe>Si>Ti>Cu>Mg>Cr>Mn。总体来说, 所有元素的ARE值为14.45%, 说明通过本方法基本能准确、快速地分析出物质中多种元素的含量情况。
2.3 市售铝箔纸样品检测结果
27 种铝箔纸样品的8种微量元素检测结果见表6, 如表所示, Cr、Mg、Mn、Zn元素均未检出, Cu、Ti元素检出频率较低, Fe、Si元素检出频率较高, 几乎所有样品都有测出。为了更好的观察各微量元素的检出情况, 将各元素在所有样品中的数值进行平均并计算其标准偏差, 结果如图8所示。可以看出Fe、Si含量是最高的元素, 其在各样品中的检出频率也较高, 而相较之下, Cu和Ti的含量非常低; 其次, 重金属Cr全部未检出, 说明市售铝箔纸安全性较高; 另一方面, 所有检出元素的标准偏差均较大, 说明不同样品中各元素的含量差异较大, 可能不同厂商在制造过程中使用了不同的工艺。
3 讨论与结论
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铝箔纸作为一种由高纯度铝经精密冷轧工艺制成的超薄金属箔材, 其近乎完美的阻隔性能(气体、水汽、光线、气味)、突出的热反射特性、良好的机械加工适应性、可靠的化学稳定性和卫生安全性, 以及优异的可回收性, 成为一种在食品包装中不可或缺的关键功能材料。尤其在需要长期保护内容物品质免受环境因素(氧、湿、光、热、微生物)侵蚀的应用场景中, 是其他单一材料难以替代的。生活中多场景、高频率的应用使产品的安全性越来越受到人们的重视。铝箔的生产工艺对其元素含量, 尤其是有害元素具有显著影响, 这直接关系到最终产品的食品安全性与材料性能。在铝箔生产中常添加少量合金元素(如Fe、Si、Mn、Cu)以优化性能, Fe和Si是常见的杂质元素, 相关研究发现, Si与Fe形成Al-Fe-Si相, 可改善耐高温性能[34]。本研究中所有样品Fe、Si检出的含量最高, Cu、Ti检出频率较低, Cr、Mg、Mn、Zn均未检出, 检测结果显示目前市售产品基本符合国家安全标准, 与国家质量检测结果相符。
目前检测常用的原子光谱或质谱类仪器, 需要用强酸酸消解样品, 不环保、实验耗时且仪器成本较高。本研究基于FL-LIBS, 优化开发了一套铝箔纸中微量元素的快速检测方法, 该方法无需样品制备, 分析速度快, 成本低廉, 在标准物质的检测中各元素的分析灵敏度均较高, LOD较低。未来在铝制食品包装乃至其他食品中元素的快速检测有很好的应用前景。但本研究亦存在一些缺陷, 与课题组前期实验方法中使用的激光器型号、光谱仪通道数以及实验参数均不同, 使得检出效果有差异, 且两个研究中使用的样品也不同, 造成了实验结果的差异。本研究中非金属元素Si的检测灵敏度较低, 系该元素相对的光谱激发惰性所致; 另外检测的相对标准偏差普遍10%~20%之间, 属于偏高的水平, 系由于激光与样品的作用过程较为剧烈, 包含样品在高能激光作用下的融化、蒸发、等离子体形成、扩张、等离子体光屏蔽效应所致, 造成了一定程度的检测过程的不稳定性。未来可额外引入辅助电离激发技术, 如火花放电技术、磁场约束技术等进一步优化各元素的检测灵敏度和LOD, 并通过进一步优化实验装置和条件提高分析的精确度, 以期将其应用在更多样品种类的分析检测中。
基金
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  • 福建省自然科学基金项目(2022J0123)
  • 厦门市自然科学基金项目(3502Z20227312)
  • 厦门医学院青年引进人才培育项目(K2023-15)
  • 国家市场监督管理总局科技计划项目(2023MK135)
文献
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参考文献 引证文献
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2025年第16卷第14期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250331007
  • 接收时间：2025-03-31
  • 首发时间：2026-01-07
  • 出版时间：2025-07-25
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  • 收稿日期：2025-03-31
基金
福建省自然科学基金项目(2022J0123)
厦门市自然科学基金项目(3502Z20227312)
厦门医学院青年引进人才培育项目(K2023-15)
国家市场监督管理总局科技计划项目(2023MK135)
作者信息
    1 厦门医学院天然化妆品福建省高校工程研究中心, 厦门 361023
    2 厦门大学萨本栋微米纳米科学技术研究院, 厦门 361102
    3 广州检验检测认证集团有限公司, 广州 511447

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*张书迪(1991—), 男, 博士, 副教授, 主要研究方向为光谱分析仪器及方法的开发。E-mail:
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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